超高效液相色谱-串联质谱法同时测定小吃类食品和火锅底料中5种罂粟壳生物碱和6种工业染料

Simultaneous determination of 5 kinds of pericarpium papaveris alkaloids and 6 kinds of industrial dyes in snack foods and hot pot seasoning by ultra performance liquid chromatography-tandem mass spectromentry

目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时测定小吃类食品及火锅底料中5种罂粟壳生物碱和6种工业染料。方法样品采用乙腈溶液提取,乙腈层经无水硫酸镁脱水后于40℃下旋转蒸发浓缩至干,用2.0 mL乙腈+0.1%甲酸水(95:5,V:V)溶解残渣,样液过膜后经C_(18)柱分离,电喷雾正、负离子同时扫描模式下多反应监测方式检测,外标法定量。结果 5种罂粟壳生物碱和6种工业染料在2.5~100μg/L的浓度范围内,具有良好的线性关系(相关系数均大于0.9980),在3个添加水平下样品的平均回收率为72.2%~108%,相对标准偏差2.5%~9.6%,罂粟碱、那可丁、蒂巴因、玫瑰红B、酸性橙Ⅱ、碱性嫩黄O、碱性黄1的检出限为1.0μg/kg,吗啡、可待因、碱性橙Ⅱ、苏丹红Ⅳ的检出限为2.5μg/kg。实际样品检测中,检出酸性橙Ⅱ阳性样品6个,含量为0.00706~74.2 mg/kg。结论该方法准确、灵敏、快速,是同时检测小吃类食品和火锅底料中罂粟壳生物碱和工业染料的有效方法。

Objective To establish a method for simultaneous determination of 5 kinds of pericarpium papaveris alkaloids and 6 kinds of industrial dyes in snack foods and hot pot seasoning by ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. Methods The samples were extracted with acetonitrile, acetonitrile layer were condensed to dry at 40℃ after dehydration of anhydrous magnesium sulfate, then 2.0 mL solution containing acetonitrile and 0.1% firnue acid （95：5, V：V） were added into the residue. After through the millipore membrane, the samples were separated on a C18 column, detected by UPLC- MS/MS, identified by electrospray ionization in positive and negative mode under multiple reaction monitoring mode, and quantified by the external standard method. Results The linear range of the method was 2.5-100 ~tg/L with the linear correlation coefficients above 0.9980. The average recoveries were from 72.2% to 108% at the 3 spiked levels, and the relative standard deviations were between 2.5% and 9.6%. The limits of detection were 1.0 ~tg/kg for papaverine, narcotine, thebaine, rhodamine B, orange II, auramine O, thioflavine T, and 2.5 ixg/kg for morphine, codeine, sudan IV. Six samples were detected of orange II from 0.00706 to 74.2 mg/kg in actual samples test. Conclusion This method is accurate and sensitive, which is an effective method for simultaneous determination of 5 kinds of alkaloids extracted from pericarpium papaveris and 6 kinds of industrial dyes in snack foods and hot pot seasoning.